Glass comprising solid electrolyte particles and lithium battery

Patent metadata

Field	Value
Publication number	US-11431024-B2
Application number	US-202117153996-A
Country	US
Kind code	B2
Filing date	Jan 21, 2021
Priority date	Apr 10, 2009
Publication date	Aug 30, 2022
Grant date	Aug 30, 2022

Abstract

A method for producing a solid electrolyte, including: stirring a slurry including lithium sulfide and phosphorus sulfide in a hydrocarbon solvent in a reaction vessel, and circulating the slurry through a connecting pipe by a pump. The method is carried out in an apparatus including the reaction vessel and the connecting pipe connected to the pump and the reaction vessel.

First claim

The invention claimed is:

1. A method for producing a solid electrolyte, the method comprising:
stirring a slurry comprising lithium sulfide and phosphorus sulfide in a hydrocarbon solvent in a reaction vessel; and
circulating the slurry through a connecting pipe by a pump,
wherein the stirring and the circulating are carried out in an apparatus comprising the reaction vessel and the connecting pipe connected to the pump and the reaction vessel.

2. The method of claim 1 , wherein a reaction temperature in the reaction vessel is 60 to 300° C.

3. The method of claim 1 , wherein a reaction temperature in the reaction vessel is 80 to 200° C.

4. The method of claim 1 , wherein the phosphorus sulfide is phosphorus pentasulfide (P 2 S 5 ).

5. The method of claim 4 , wherein a molar ratio of the lithium sulfide to the phosphorus pentasulfide is from 50:50 to 80:20.

6. The method of claim 4 , wherein a molar ratio of the lithium sulfide to the phosphorus pentasulfide is from 60:40 to 75:25.

7. The method of claim 1 , wherein the hydrocarbon solvent comprises at least one selected from the group consisting of a saturated hydrocarbon, an unsaturated hydrocarbon, and an aromatic hydrocarbon.

8. The method of claim 1 , wherein the hydrocarbon solvent comprises an aromatic hydrocarbon.

9. The method of claim 1 , wherein the hydrocarbon solvent comprises toluene, xylene, or both.

10. The method of claim 1 , wherein a heat exchanger is provided to the connecting pipe.

11. The method of claim 10 , further comprising:
cooling the slurry extracted from the reaction vessel by the heat exchanger.

12. The method of claim 1 , wherein a grinder is provided to the connecting pipe, the grinder configured to grind the lithium sulfide and the phosphorus sulfide.

13. The method of claim 12 , wherein the grinder is a rotary mill, a swing mill, a vibration mill, or a bead mill.

14. The method of claim 1 , wherein a reaction time in the reaction vessel is 5 minutes to 50 hours.

15. The method of claim 1 , wherein a reaction time in the reaction vessel is 10 minutes to 40 hours.

16. The method of claim 1 , wherein a heat exchanger and a grinder are provided to the connecting pipe such that the heat exchanger is positioned between the reaction vessel and the grinder.

17. The method of claim 1 , wherein the hydrocarbon solvent has a water content of 50 ppm by weight or less.

18. The method of claim 1 , wherein the hydrocarbon solvent has a water content of 20 ppm by weight or less.

19. The method of claim 1 , further comprising:
drying a reaction product obtained by the stirring and the circulating such that the hydrocarbon solvent is removed from the reaction product.

20. The method of claim 1 , wherein when a Raman spectrum of the solid electrolyte is repeatedly measured and a peak at 330 to 450 cm −1 in each Raman spectrum is separated to waveforms of individual components, a standard deviation of a waveform area ratio of each component is less than 4.0.

Assignees

• Idemitsu Kosan Co

Inventors

• Aburatani Ryo
• Senga Minoru
• Ota Tsuyoshi
• Nakagawa Masaru

Classifications

• H01M10/0562 Primary

  Solid materials · CPC title

• C03C12/00

  Powdered glass (C03C8/02 takes precedence); Bead compositions · CPC title

• H01M4/62

  Selection of inactive substances as ingredients for active masses, e.g. binders, fillers · CPC title

• C03B2201/86

  Chalcogenide glasses, i.e. S, Se or Te glasses · CPC title

• C03C1/02

  Pretreated ingredients · CPC title